Preparation method of efficient polypropylene flame-retardant synergistic master batch

Abstract

The invention discloses a preparation method of an efficient polypropylene flame-retardant synergistic master batch, and relates to the technical field of high polymer materials, and the preparation method is as follows: glyceryl stearate and polyolefin are uniformly mixed to form a mixture, and the mixture is extruded by a twin-screw extruder to prepare the efficient polypropylene flame-retardant synergistic master batch; the polyolefin is any one or more of polypropylene of 1100N, polypropylene of K7227H or polypropylene of RE420MO; the glyceryl stearate is any one or more of tripolyglyceryl monostearate, decapolyglyceryl stearate, diisostearin, tripolyglyceryl distearate and hexapolyglyceryl pentastearate; the polyglyceryl stearate is any one or more of tripolyglyceryl monostearate, decapolyglyceryl stearate, diisostearin, tripolyglyceryl distearate and hexapolyglyceryl pentastearate; according to the invention, polypropylene is used as matrix resin, glyceryl stearate is used as an additive for blending extrusion to prepare the flame-retardant synergistic master batch, and the aim of improving the performance of the halogen-free flame-retardant polypropylene material is fulfilled by using the characteristics of self-lubrication, dispersion assistance and flame retardance assistance of glyceryl stearate.

Description

Technical Field

[0001] The invention relates to the technical field of polymer materials, and in particular to a method for preparing a high-efficiency polypropylene flame-retardant synergistic masterbatch. Background Art

[0002] As one of the five general materials, polypropylene (PP) is widely used in daily life and industrial production such as automobiles, home appliances, construction, medicine, food packaging, etc. due to its good performance, low density, chemical corrosion resistance and flex resistance. However, with the widespread application of poly PP, a large number of safety hazards have also emerged. Among them, the flammability of PP is one of the important reasons for major production and life safety accidents.

[0003] At present, the flame retardants used in PP industrial production mainly include phosphorus flame retardants, halogen flame retardants and inorganic hydroxides. Among them, halogen flame retardants have become the main flame retardant additives due to their excellent flame retardant efficiency and simple processing methods. However, they will produce a large amount of toxic and corrosive gases during the combustion process, which makes the large-scale use of halogen flame retardants no longer in line with the current green, environmentally friendly and sustainable development concepts. The halogen-free flame retardant system has the problems of narrow processing window and poor performance of the prepared materials, so it is usually necessary to toughen the material in the preparation of flame-retardant PP. Summary of the invention

[0004] The purpose of the present invention is to provide a method for preparing a high-efficiency polypropylene flame retardant synergistic masterbatch; to solve the following technical problems:

[0005] 1) Uneven dispersion of flame retardants: It is difficult to evenly disperse the flame retardants in the halogen-free flame retardant system, which affects the flame retardant effect;

[0006] 2) Insufficient protection of glass fiber: During the preparation process, glass fiber is easily damaged, affecting the overall performance of the material;

[0007] 3) Difficulty in improving material performance: The performance of materials prepared by halogen-free flame retardant systems is poor and it is difficult to meet application requirements.

[0008] The purpose of the present invention can be achieved by the following technical solutions:

[0009] In the first aspect, the present invention discloses a method for preparing a high-efficiency polypropylene flame retardant synergistic masterbatch, and the preparation method is as follows:

[0010] Glyceryl stearate and polyolefin are uniformly mixed to form a mixture, and the mixture is extruded by a twin-screw extruder to prepare the high-efficiency polypropylene flame retardant synergistic masterbatch.

[0011] Preferably, the polyolefin is any one or more of 1100N polypropylene, K7227H polypropylene or RE420MO polypropylene.

[0012] Preferably, the stearin is any one or more of triglycerol monostearate, decaglycerol stearate, diisostearate, triglycerol distearate, and hexaglycerol pentastearate.

[0013] Preferably, in the mixture, polyolefin accounts for 30%-70%, and glyceryl stearate accounts for 30%-70%.

[0014] Preferably, the temperature of the twin-screw extruder is 170-220° C., and the rotation speed is 120-350 r / min.

[0015] In a second aspect, the present invention further discloses a halogen-free flame-retardant polypropylene, the components of which include the flame-retardant synergistic masterbatch as described above, and the component proportion of the flame-retardant synergistic masterbatch is 0.2%-10%.

[0016] Beneficial effects of the present invention:

[0017] (1) The present invention uses polyolefin as a base resin and glyceryl stearate as an additive to prepare a flame retardant synergistic masterbatch by blending and extruding, and utilizes the self-lubricating, dispersing and flame retardant characteristics of glyceryl stearate itself to achieve the purpose of improving the performance of halogen-free flame retardant polypropylene materials;

[0018] (2) The present invention is applicable to a variety of homopolymers, copolymers of PP and polyethylene, and has high universality;

[0019] (3) The raw materials used in the present invention are low in price, the preparation method is simple, and it is suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The present invention will be further described below in conjunction with the accompanying drawings.

[0021] Figure 1 This is a schematic diagram of the glass fiber length of halogen-free flame-retardant polypropylene before adding the synergistic masterbatch;

[0022] Figure 2 This is a schematic diagram of the glass fiber length of halogen-free flame-retardant polypropylene after adding synergistic masterbatch. DETAILED DESCRIPTION

[0023] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] The experimental raw materials involved in the following examples are: homopolypropylene (1100N, Shenhua Ningmei), copolymer polypropylene (K7227H, Wuhan Petrochemical or RE420MO, Borealis Chemical), triglycerol monostearate (Jiangsu Caiwei), decaglycerol stearate (Jinsheng New Materials), diisostearate (Anhui Hongrui Biology), triglycerol distearate (Jiangsu Caiwei), and hexaglycerol pentastearate (Lanabai).

[0025] Example 1

[0026] Preparation of flame retardant synergistic masterbatch:

[0027] 50 wt% 1100N polypropylene and 50 wt% triglycerol monostearate were put into a blender and mixed evenly to obtain a mixture; the mixture was poured into a 200° C., 200 r / min twin-screw extruder, and flame retardant synergistic masterbatch was prepared by extrusion, cooling, and pelletizing;

[0028] Preparation of halogen-free flame-retardant polypropylene:

[0029] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 2wt% polyolefin elastomer, 1wt% antioxidant, and 5wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 25wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0030] Example 2

[0031] Preparation of flame retardant synergistic masterbatch:

[0032] 30 wt% 1100N polypropylene and 70 wt% triglycerol monostearate were put into a blender and mixed evenly to obtain a mixture; the mixture was poured into a twin-screw extruder at 170° C. and 350 r / min, and flame retardant synergistic masterbatch was prepared by extrusion, cooling and pelletizing;

[0033] Preparation of halogen-free flame-retardant polypropylene:

[0034] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 1.8wt% polyolefin elastomer, 1wt% antioxidant, and 0.2wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 30wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0035] Example 3

[0036] Preparation of flame retardant synergistic masterbatch:

[0037] 70 wt% 1100N polypropylene and 30 wt% triglycerol monostearate were put into a blender and mixed evenly to obtain a mixture; the mixture was poured into a twin-screw extruder at 220° C. and 120 r / min, and flame retardant synergistic masterbatch was prepared by extrusion, cooling and pelletizing;

[0038] Preparation of halogen-free flame-retardant polypropylene:

[0039] 45wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 1.8wt% polyolefin elastomer, 1wt% antioxidant, and 10wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 25wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0040] Example 4

[0041] Preparation of high-efficiency polypropylene flame retardant synergistic masterbatch:

[0042] 30 wt% K7227H polypropylene and 70 wt% polyglycerol stearate were put into a blender and mixed evenly to obtain a mixture; the mixture was poured into a twin-screw extruder at 220° C. and 120 r / min, and flame retardant synergistic masterbatch was prepared by extrusion, cooling, and pelletizing;

[0043] Preparation of halogen-free flame-retardant polypropylene:

[0044] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 2wt% polyolefin elastomer, 1wt% antioxidant, and 5wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 25wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0045] Example 5

[0046] Preparation of flame retardant synergistic masterbatch:

[0047] 30 wt% RE420MO polypropylene and 70 wt% polyglycerol stearate were put into a blender and mixed evenly to obtain a mixture; the mixture was poured into a twin-screw extruder at 220° C. and 120 r / min, and flame retardant synergistic masterbatch was prepared by extrusion, cooling, and pelletizing;

[0048] Preparation of halogen-free flame-retardant polypropylene:

[0049] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 2wt% polyolefin elastomer, 1wt% antioxidant, and 5wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 25wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0050] Example 6

[0051] Preparation of flame retardant synergistic masterbatch:

[0052] 70 wt% RE420MO polypropylene and 30 wt% polyglycerol stearate are put into a blender and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder at 220° C. and 120 r / min, and a flame retardant synergistic masterbatch is prepared by extrusion, cooling, and pelletizing;

[0053] Preparation of halogen-free flame-retardant polypropylene:

[0054] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 2wt% polyolefin elastomer, 1wt% antioxidant, and 5wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 25wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0055] Example 7

[0056] Preparation of flame retardant synergistic masterbatch:

[0057] 50 wt% 1100N polypropylene and 50 wt% diisostearate are put into a blender and mixed evenly to obtain a mixture; the mixture is poured into a 200° C., 200 r / min twin-screw extruder, and flame retardant synergistic masterbatch is prepared by extrusion, cooling, and pelletizing;

[0058] Preparation of halogen-free flame-retardant polypropylene:

[0059] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 2wt% polyolefin elastomer, 1wt% antioxidant, and 2wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 28wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0060] Example 8

[0061] Preparation of high-efficiency polypropylene flame retardant synergistic masterbatch:

[0062] Preparation of flame retardant synergistic masterbatch:

[0063] 30wt% 1100N polypropylene and 70wt% triglycerol distearate are put into a blender and mixed evenly to obtain a mixture; the mixture is poured into a 200°C, 200r / min twin-screw extruder, and flame retardant synergistic masterbatch is prepared by extrusion, cooling and pelletizing;

[0064] Preparation of halogen-free flame-retardant polypropylene:

[0065] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 2wt% polyolefin elastomer, 1wt% antioxidant, and 2wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 28wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0066] Example 9

[0067] Preparation of high-efficiency polypropylene flame retardant synergistic masterbatch:

[0068] Preparation of flame retardant synergistic masterbatch:

[0069] 30 wt% 1100N polypropylene and 70 wt% hexaglycerol pentastearate were put into a blender and mixed evenly to obtain a mixture; the mixture was poured into a twin-screw extruder at 170° C. and 350 r / min, and flame retardant synergistic masterbatch was prepared by extrusion, cooling, and pelletizing;

[0070] Preparation of halogen-free flame-retardant polypropylene:

[0071] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 2wt% polyolefin elastomer, 1wt% antioxidant, and 2wt% of the flame-retardant shoe synergistic masterbatch prepared above are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 28wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling, and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0072] Comparative Example 1

[0073] Preparation of halogen-free flame-retardant polypropylene:

[0074] 50wt% 1100N polypropylene, 17wt% ammonium polyphosphate, 2wt% polyolefin elastomer and 1wt% antioxidant are put into a high mixing pot and mixed evenly to obtain a mixture; the mixture is poured into a twin-screw extruder, and 30wt% glass fiber is poured into the side of the twin-screw extruder at the same time, and extrusion, cooling and pelletizing are performed to prepare sample particles; the pellets are placed in an injection molding machine at 180°C for injection molding to obtain halogen-free flame-retardant polypropylene.

[0075] The halogen-free flame-retardant polypropylene obtained in Examples 1-9 and Comparative Example 1 was subjected to mechanical property tests and flame retardant property tests, and the test methods were as follows:

[0076] Tensile strength: Refer to GB / T 1040

[0077] Bending strength: Refer to GB / T 9341

[0078] Cantilever beam notch: refer to GB / T 1843

[0079] Vertical combustion level: Refer to UL94

[0080] The test results are listed in Table 1. Table 1 is as follows:

[0081] Table 1

[0082] Tensile strength(Mpa) Bending strength(Mpa) <![CDATA[Izod impact strength of cantilever beam (kJ / m 2 )]]> Vertical burning level Example 1 79.4 122.9 13.9 V0 Example 2 78.8 124.1 129 V0 Example 3 79.9 122.6 13.4 V0 Example 4 80.1 123.8 14.1 V0 Example 5 78.9 123.4 14.4 V0 Example 6 79.8 122.8 13.5 V0 Example 7 80.4 120.9 13.7 V0 Example 8 78.9 125.1 14.2 V0 Example 9 80.3 124.6 14.1 V0 Comparative Example 1 79.1 121.8 11.2 V1

[0083] By analyzing the data in Table 1, it can be known that the halogen-free flame retardant polypropylene prepared in Examples 1-9 has higher tensile strength, flexural strength and cantilever beam notched impact than that in Comparative Example 1, and has a higher flame retardant grade, which indicates that the addition of the flame retardant synergistic masterbatch enhances the mechanical strength and flame retardant properties of the halogen-free flame retardant polypropylene.

[0084] The morphology of the halogen-free flame-retardant polypropylene of Example 1 and Comparative Example 1 was detected, and the results were as follows: Figure 1-2 The morphology of Figure 1It can be seen that the average length of the glass fiber of the halogen-free flame-retardant polypropylene added with the flame-retardant synergistic masterbatch in Example 1 is 226um. Figure 2 It can be seen that the average glass fiber length of the halogen-free flame retardant polypropylene in Comparative Example 1 without the addition of the flame retardant synergistic masterbatch is 197 um; this indicates that the addition of the flame retardant synergistic masterbatch prolongs the average glass fiber length of the halogen-free flame retardant polypropylene, thereby enhancing its performance.

[0085] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A method for preparing a flame retardant synergistic masterbatch, characterized in that: The preparation method is as follows: Glyceryl stearate and polyolefin are uniformly mixed to form a mixture, and the mixture is extruded by a twin-screw extruder to prepare the high-efficiency polypropylene flame retardant synergistic masterbatch.

2. The method for preparing the flame retardant synergistic masterbatch according to claim 1, characterized in that: The stearin is a mixture of any one or more of triglycerol monostearate, decaglycerol stearate, diisostearate, triglycerol distearate, and hexaglycerol pentastearate.

3. The method for preparing the flame retardant synergistic masterbatch according to claim 1, characterized in that: The polyolefin is a mixture of any one or more of 1100N polypropylene, K7227H polypropylene, and RE420MO polypropylene.

4. The method for preparing the flame retardant synergistic masterbatch according to claim 1, characterized in that: In the mixture, polyolefin accounts for 30%-70%, and the remainder is glyceryl stearate.

5. The method for preparing the flame retardant synergistic masterbatch according to claim 1, characterized in that: The temperature of the twin-screw extruder is 170-220° C., and the rotation speed is 120-350 r / min.

6. A halogen-free flame-retardant polypropylene, characterized in that: Its components include the flame retardant synergistic masterbatch described in any one of claims 1 to 5, and the proportion of the flame retardant synergistic masterbatch is 0.2%-10%.

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